Grain Refinement at the Nanoscale Via Mechanical Twinning and Dislocation Interaction in a Nickel-Based Alloy

A nanostructured surface layer was formed on an Inconel 600 plate by subjecting it to surface mechanical attrition treatment at room temperature. Transmission electron microscopy and high-resolution transmission electron microscopy of the treated surface layer were carried out to reveal the underlying grain refinement mechanism. Experimental observations showed that the strain-induced nanocrystallization in the current sample occurred via formation of mechanical microtwins and subsequent interaction of the microtwins with dislocations in the surface layer. The development of high-density dislocation arrays inside the twin-matrix lamellae provides precursors for grain boundaries that subdivide the nanometer-thick lamellae into equiaxed, nanometer-sized grains with random orientations.

Laser-surface-alloyed carbon nanotubes reinforced hydroxyapatite composite coatings

Carbon-nanotube sCNTd-reinforced hydroxyapatite composite coatings have been fabricated by laser surface alloying. Microstructural observation using high-resolution transmission electron microscopy showed that a large amount of CNTs remained with their or

Laser microstructuring of Si surfaces for low-threshold field-electron emission

Dense arrays of high aspect ratio Si micro-pyramids have been formed by cumulative high intensity laser irradiation of doped Si wafers in an SF6 environment. A comparative study using nanosecond (XeCl, 308 nm) and femtosecond (Ti: Sapphire, 800 nm and KrF, 248 nm) laser pulses has been performed in this work. The influence of pulse duration and ambient gas pressure (SF6) is also presented. Scanning electron microscopy has shown that upon laser irradiation conical features appear on the Si surface in a rather homogenous distribution and with a spontaneous self alignment into arrays. Their lowest tip diameter is 800 nm; while their height reaches up to 90 mum. Secondary tip decoration appears on the surface of the formed spikes. Areas of 2 X 2 mm(2) covered with Si cones have been tested as cold cathode field emitters. After several conditioning cycles, the field emission threshold for the studied Si tips is as low as 2 V/mum, with an emission current of 10(-3) A/cm(2) at 4 V/mum. Even though these structures have smaller aspect ratios than good quality carbon nanotubes, their field emission properties are similar. The simple and direct formation of field emission Si arrays over small pre-selected areas by laser irradiation could lead to a novel approach for the development of electron sources. (C) 2003 Elsevier B.V. All rights reserved.

The effect of carbon encapsulation on the magnetic properties of Ni nanoparticles produced by arc discharge in de-ionized water

Despite intensive research on optimizing the methods for depositing carbon encapsulated ferromagnetic nanoparticles, the effect of the carbon cages remains unclear. In the present work, the effect of the graphitic cages on the magnetization of the ferromagnetic core has been studied by comparing the magnetic properties of pure and carbon encapsulated Ni particles of the same size. The carbon encapsulated Ni particles were formed using an electric arc discharge in de-ionized water between a solid graphite cathode and an anode consisting of Ni and C in a mass ratio of Ni:C = 7:3. This method is shown to have potential for low cost production of carbon encapsulated Ni nanoparticle samples with narrow particle size distributions. X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM) analysis were used to study the crystallography, morphology, and size distribution of the encapsulated and pure Ni nanoparticle samples. The availability of encapsulated particles with various sizes allowed us to elucidate the role of carbon cages in size-dependent properties. Our data suggest that even though encapsulation is beneficial for protection against hostile chemical environments and for avoiding low proximity phenomena, it suppresses the saturation magnetization of the Ni cores.

Deformation Defects in Nanocrystalline Nickel

Defects induced by plastic deformation in electrodeposited, fully dense nanocrystalline (nc) Ni with an average grain size of 25 nm have been characterized by means of high resolution transmission electron microscopy. The nc Ni was deformed under uniaxial tension at liquid-nitrogen temperature. Trapped full dislocations were observed in the grain interior and near the grain boundaries. In particular, these dislocations preferred to exist in the form of dipoles. Deformation twinning was confirmed in nc grains and the most proficient mechanism is the heterogeneous nucleation via emission of partial dislocations from the grain boundaries.

The role of the catalytic particle in the growth of carbon nanotubes by plasma enhanced chemical vapor deposition

Vertically aligned carbon nanotubes were synthesized by plasma enhanced chemical vapor deposition using nickel as a metal catalyst. High resolution transmission electron microscopy analysis of the particle found at the tip of the tubes reveals the presence of a metastable carbide Ni3C. Since the carbide is found to decompose upon annealing at 600 degreesC, we suggest that Ni3C is formed after the growth is stopped due to the rapid cooling of the Ni-C interstitial solid solution. A detailed description of the tip growth mechanism is given, that accounts for the composite structure of the tube walls. The shape and size of the catalytic particle determine the concentration gradient that drives the diffusion of C atoms across and though the metal. (C) 2004 American Institute of Physics.

Formation of nanoparticles from ultrafast laser condensates of metal targets

Optimised ultrafast laser ablation can result in almost complete ionisation of the target material and the formation of a high velocity plasma jet. Collisions with the ambient gas behind the shock front cools the material resulting in the formation of mainly spherical, single crystal nanoscale particles in the condensate. This work characterises the nanoscale structures produced by the ultrafast laser interactions in He atmospheres at STP with Ni and Al. High resolution transmission electron microscopy was employed to study the microstructure of the condensates and to classify the production of particles forms as a function of the illumination conditions.

Phase Evolution and its Effect on Magnetic Properties of Nd60Al10Fe20Co10 Bulk Metallic Glass

The thermal stability of nanocrystalline clusters, the phase evolution, and their effects on magnetic Propertieswere studied for as-cast Nd60Al10Fe20Co10 alloy using differential scanning calorimetry curves, x-ray diffraction patterns, scanning electron microscopy, and high-resolution transition electron microscopy. Thermomagnetic curves and hysteresis loops of the bulk metallic glass were measured during the annealing process. The high thermostability of the hardmagnetic properties of the samples observed is attributed to the stability of the nanocrystalline clusters upon annealing, while the slight enhancement in the magnetization is due to the precipitation of some Nd-rich metastable phases. The mechanism of thermostability of the nanocrystalline clusters and the formation of the metastable phases are discussed.

Fracture Mechanisms And Size Effects Of Brittle Metallic Foams: In Situ Compression Tests Inside Sem

In situ compressive tests on specially designed small samples made from brittle metallic foams were accomplished in a loading device equipped in the scanning electron microscopy (SEM). Each of the small samples comprises only several cells in the effective test zone (ETZ), with one major cell in the middle. In such a system one can not only obtain sequential collapse-process images of a single cell and its cell walls with high resolution, but also correlate the detailed failure behaviour of the cell walls with the stress-strain response, therefore reveal the mechanisms of energy absorption in the mesoscopic scale. Meanwhile, the stress-strain behaviour is quite different from that of bulk foams in dimensions of enough large, indicating a strong size effect. According to the in situ observations, four failure modes in the cell-wall level were summarized, and these modes account for the mesoscopic mechanisms of energy absorption. Paralleled compression tests on bulk samples were also carried out, and it is found that both fracturing of a single cell and developing of fracture bands are defect-directed or weakness-directed processes. The mechanical properties of the brittle aluminum foams obtained from the present tests agree well with the size effect model for ductile cellular solids proposed by Onck et al. (C) 2008 Elsevier Ltd. All rights reserved.

Avances analíticos en la datación forense de tintas y documentos

380 p. : il., gráf.

Metrologia de instrumentos endodônticos por microscopia eletrônica de varredura e análise digital de imagens: uma proposta metodológica

A padronização para a fabricação de instrumentos endodônticos em aço inoxidável contribuiu para o desenvolvimento de novos aspectos geométricos. Surgiram propostas de alterações no desenho da haste helicoidal, da seção reta transversal, da ponta, da conicidade e do diâmetro na extremidade (D0). Concomitantemente, o emprego de ligas em Níquel-Titânio possibilitou a produção de instrumentos acionados a motor, largamente empregados hoje. A cada ano a indústria lança instrumentos com diversas modificações, sem, contudo, disponibilizar informações suficientes quanto às implicações clínicas destas modificações. Existe um crescente interesse no estudo dos diferentes aspectos geométricos e sua precisa metrologia. Tradicionalmente, a aferição de aspectos geométricos de instrumentos endodônticos é realizada visualmente através de microscopia ótica. Entretanto, esse procedimento visual é lento e subjetivo. Este trabalho propõe um novo método para a metrologia de instrumentos endodônticos baseado no microscópio eletrônico de varredura e na análise digital das imagens. A profundidade de campo do MEV permite obter a imagem de todo o relevo do instrumento endodôntico a uma distância de trabalho constante. Além disso, as imagens obtidas pelo detector de elétrons retro-espalhados possuem menos artefatos e sombras, tornando a obtenção e análise das imagens mais fáceis. Adicionalmente a análise das imagens permite formas de mensuração mais eficientes, com maior velocidade e qualidade. Um porta-amostras específico foi adaptado para obtenção das imagens dos instrumentos endodônticos. Ele é composto de um conector elétrico múltiplo com terminais parafusados de 12 pólos com 4 mm de diâmetro, numa base de alumínio coberta por discos de ouro. Os nichos do conector (terminais fêmeas) têm diâmetro apropriado (2,5 mm) para o encaixe dos instrumentos endodônticos. Outrossim, o posicionamento ordenado dos referidos instrumentos no conector elétrico permite a aquisição automatizada das imagens no MEV. Os alvos de ouro produzem, nas imagens de elétrons retro-espalhados, melhor contraste de número atômico entre o fundo em ouro e os instrumentos. No porta-amostras desenvolvido, os discos que compõem o fundo em ouro são na verdade, alvos do aparelho metalizador, comumente encontrados em laboratórios de MEV. Para cada instrumento, imagens de quatro a seis campos adjacentes de 100X de aumento são automaticamente obtidas para cobrir todo o comprimento do instrumento com a magnificação e resolução requeridas (3,12 m/pixel). As imagens obtidas são processadas e analisadas pelos programas Axiovision e KS400. Primeiro elas são dispostas num campo único estendido de cada instrumento por um procedimento de alinhamento semi-automático baseado na inter-relação com o Axiovision. Então a imagem de cada instrumento passa por uma rotina automatizada de análise de imagens no KS400. A rotina segue uma sequência padrão: pré-processamento, segmentação, pós-processamento e mensuração dos aspectos geométricos.

Heteroepitaxy of Group IV and Group III-V semiconductor alloys for photovoltaic applications

Photovoltaic energy conversion represents a economically viable technology for realizing collection of the largest energy resource known to the Earth -- the sun. Energy conversion efficiency is the most leveraging factor in the price of energy derived from this process. This thesis focuses on two routes for high efficiency, low cost devices: first, to use Group IV semiconductor alloy wire array bottom cells and epitaxially grown Group III-V compound semiconductor alloy top cells in a tandem configuration, and second, GaP growth on planar Si for heterojunction and tandem cell applications.

Metal catalyzed vapor-liquid-solid grown microwire arrays are an intriguing alternative for wafer-free Si and SiGe materials which can be removed as flexible membranes. Selected area Cu-catalyzed vapor-liquid solid growth of SiGe microwires is achieved using chlorosilane and chlorogermane precursors. The composition can be tuned up to 12% Ge with a simultaneous decrease in the growth rate from 7 to 1 μm/min^-1. Significant changes to the morphology were observed, including tapering and faceting on the sidewalls and along the lengths of the wires. Characterization of axial and radial cross sections with transmission electron microscopy revealed no evidence of defects at facet corners and edges, and the tapering is shown to be due to in-situ removal of catalyst material during growth. X-ray diffraction and transmission electron microscopy reveal a Ge-rich crystal at the tip of the wires, strongly suggesting that the Ge incorporation is limited by the crystallization rate.

Tandem Ga_1-xIn_xP/Si microwire array solar cells are a route towards a high efficiency, low cost, flexible, wafer-free solar technology. Realizing tandem Group III-V compound semiconductor/Si wire array devices requires optimization of materials growth and device performance. GaP and Ga_1-xIn_xP layers were grown heteroepitaxially with metalorganic chemical vapor deposition on Si microwire array substrates. The layer morphology and crystalline quality have been studied with scanning electron microscopy and transmission electron microscopy, and they provide a baseline for the growth and characterization of a full device stack. Ultimately, the complexity of the substrates and the prevalence of defects resulted in material without detectable photoluminescence, unsuitable for optoelectronic applications.

Coupled full-field optical and device physics simulations of a Ga_0.51In_0.49P/Si wire array tandem are used to predict device performance. A 500 nm thick, highly doped "buffer" layer between the bottom cell and tunnel junction is assumed to harbor a high density of lattice mismatch and heteroepitaxial defects. Under simulated AM1.5G illumination, the device structure explored in this work has a simulated efficiency of 23.84% with realistic top cell SRH lifetimes and surface recombination velocities. The relative insensitivity to surface recombination is likely due to optical generation further away from the free surfaces and interfaces of the device structure.

Finally, GaP has been grown free of antiphase domains on Si (112) oriented substrates using metalorganic chemical vapor deposition. Low temperature pulsed nucleation is followed by high temperature continuous growth, yielding smooth, specular thin films. Atomic force microscopy topography mapping showed very smooth surfaces (4-6 Å RMS roughness) with small depressions in the surface. Thin films (~ 50 nm) were pseudomorphic, as confirmed by high resolution x-ray diffraction reciprocal space mapping, and 200 nm thick films showed full relaxation. Transmission electron microscopy showed no evidence of antiphase domain formation, but there is a population of microtwin and stacking fault defects.

Estudo da bioenergética mitocondrial de cardiomiócitos de camundongos obesos

A obesidade é uma doença crônica, resultante do excesso de gordura no organismo. O aumento da obesidade no mundo, tem se revelado como um dos fenômenos clínicos e epidemiológicos da atualidade. Estudos populacionais e em modelos animais demonstram que a origem da epidemia da obesidade está relacionada a fatores genéticos, modificações de hábitos nutricionais, redução da atividade física, e alterações nutricionais durante a lactação, desempenhando um papel relevante no desenvolvimento da obesidade, DM2 e cardiomiopatias. As mitocôndrias são os coordenadores centrais do metabolismo energético, assim, alterações funcionais e estruturais dessa organela têm sido associadas à desordens metabólicas. Elas exercem um papel na sobrevivência e função dos cardiomiócitos devido à alta demanda energética do miocárdio. Desta forma, disfunções mitocondriais estão relacionadas com disfunções no miocárdio e conseqüente progressão de cardiomiopatias. Neste estudo, avaliamos a bioenergética e a ultraestrutura de cardiomiócitos de camundongos obesos e controle hiperalimentados durante a lactação. O consumo de oxigênio das fibras cardíacas foi avaliado por respirometria de alta-resolução, utilizando um oxígrafo-2K-Oroboros. A ultraestrutura dos cardiomiócitos foi analisada por microscopia eletrônica de transmissão e o conteúdo das proteínas Carnitina palmitoil transferase 1 (CPT1), Proteína desacopladora 2 (UCP2) , Transportador de glicose 1 e 4 (GLUT1) e (GLUT4), Proteína Kinase ativada por AMP (AMPK) e Proteína kinase ativada por AMP fosforilada p(AMPK) por Western blotting (WB). Além disso, o peso dos animais, a gordura retroperitoneal, epididimal e a glicemia em jejum foram determinadas. Nossos resultados confirmaram que os animais do grupo hiperalimentados (GH), aos 90 dias de vida, apresentaram aumento da massa corporal, de gordura epididimária e retroperitoneal comparado ao grupo controle (GC). As taxas respiratórias foram semelhantes nos dois grupos quando foram utilizados os substratos dos complexos I e II. Entretanto, quando o ácido graxo palmitoil-L-carnitina foi utilizado, a taxa respiratória máxima do GH foi significativamente menor. A análise ultraestrutural dos cardiomiócitos do GH demonstrou intenso dano na matriz mitocondrial e maior presença de gotículas de lipídios, caracterizando deposição ectópica. Os resultados do WB mostraram aumento significativo do conteúdo de CPT1 e UCP2 no GH comparado ao GC. Não foram encontradas diferenças significativas no conteúdo de GLUT1 entre os grupos, entretanto, observamos maior conteúdo do GLUT4 no GH. Além disso, encontramos maior conteúdo de AMPK no GH, ao passo que o conteúdo de pAMPK foi semelhante entre os grupos. Entretanto, a razão pAMPK/AMPK é significativamente menor no GH. Esses resultados sugerem que a hiperalimentação durante a lactação leva a obesidade na vida adulta com alterações na bioenergética e ultraestrutura dos cardiomiócitos.